Apparatus for saponification and extraction



April 17, 194 5. D. s. BINNINGTON APPARATUS FOR SAPONIFICATION ANDEXTRACTION Q 2 Sheets-Sheet 1 Original Filed Jan. 13, 1941 N 5 anRMvNwOm NIQWNN Mai W lazi April 1945. D. s. BINNINGTON 2,373,646

APPARATUS FOR SAPONIFICATION AND EXTRACTION Original Filed Jan. 13, 19412 Sheets-Sheet 2 lull-incl...

v Jnveniop Dpnald J. fi z'iznin gion/ Patented Apr. 17, 1945 APPARATUSFOR SAPONIFICATION AND EXTRACTION Donald S. Binnington, St. Paul, Minn.,assignor to General Mills, Inc., a corporation of Delaware Originalapplication January 13, 1941, Serial No. 374,261. Divided and thisapplication June 30,

1941, Serial No. 400,549

4 Claims.

This is a division of my application Serial No. 374,261, filed January13, 1941.

An object of this invention is to provide apparatus for saponifyingcertain oils, particularly those containing substances subject tooxidation under normal conditions of saponification and extraction, andfor extracting non-saponifiable matter under conditions which inhibitoxidation.

Another and more particular object is to provide apparatus forrecovering from an oil, particularly a vegetable oil, a non-saponifiablesubstance containing a vitamin, for example, for recovering from wheatgerm oil a non-saponiflable concentrate containing vitamin E, whichrapidly loses its potency in the presence of alkali and air, bysaponification and extraction of the non-saponifiable substance underconditions which willpreserve the potency of the vitamin.

These and other objects as will hereinafter appear are accomplished bythis invention which is fully described in the following specificationand shown in the accompanying drawings in which the figures showdiagrammatically apparatus for practicing the invention. Figure l is anembodiment of the invention adapted to the use of a solvent lighter thanthe liquid to be extracted. Fig. 2 is a modification for the use of asolvent heavier than liquid to be extracted.

In a method of this kind we must consider the use of first a solventlighter than water and second a solvent heavier than water.

The apparatus illustrated in Fig. 1 for carrying out the first methodwith a solvent lighter than water comprises principally a treating tankl0, a boiler II for solvent, a condenser l2, and

a gas holder l3, these being connected by suit-' able piping which willnow be described. The gas holder is maintained under a predeterminedslightly super-atmospheric pressure by any well known means. The top ofthe boiler for solvent is connected with the top of the tank by arelatively large pipe I6 having therein a control valve IT. A vaporlinel8 also connects the top of the boiler for solvent through condensertubes 20 in the condenser I 2, a valve 2| and pipe 22 and 22 to aperforated coil or the like I 23 in the bottom of the tank. Theseperforations enable the solvent to bubble up through the entire body ofliquid in the tank. A vent I! may be provided to assist in the removalof air from the system prior to the beginning of operations as willappear more fully hereinafter.

The top of the condenser l2 connects through a pipe 24 with a controlvalve 25 therein with the gas holder II, the latter preferably having asuitable counter-weight 26. Liquids may be admitted to the tankthrough apipe 30 having a valve 3| therein, and this tank is provided with adrain controlled by a valve 32. The boiler II is similarly provided witha' drain having a control valve 33 which may also serve for admission ofliquids to the boiler. The bottom of the condenser is connected to thetop of the tank by a large reflux line l9 controlled by a valve 36. Apressure equalizing line 34 having a valve 35 connects pipe 24 to pipe22. The connection 22 from line i9 to pipe 22 should be of largediameter in order to prevent plugging the system with condensed liquid.

The bottom of the tank is provided with a steam or hot water jacket 31and the boiler II is heated as by means of steam coils 38. In this firstform, the solvent must be lighter than water in order to effectextraction by separation and may be ethyl ether, petroleum distillate,or similar oil solvents lighter than water and not readily miscibletherewith at ordinary temperatures. If some of the solvent does becomedissolved in the water in the tank, saturation is soon reached afterwhich the solvent floats on the water with a sharply defined level.

The method of operation of this first method is as follows: Theapparatus is completely filled with water and as this is drained ofithrough the drain valves 32 and 33, nitrogen, or a similar inert gas, isadmitted to the system from the gas holder I3 at a slightlysuperatmospheric pressure and until the apparatus is completely filledwith this inert gas. When this is accomplished, I pump into the tank Hithe oil to be treated, such as wheat germ oil containing vitamin E, anda suitable alkali solution in proper volume and proportions forsaponification. Hot water or steam is introduced to the jacket 31 toheat the mixture of oil and alkali solution, and saponification isaccomplished by thus boiling this mixture. During this operation, valvesll, 2|, 31, 32, 33 and 35 are closed while valves 25 and 36 remain openso that any vapors distilled off will be condensed and returned to thetank.

After saponiflcation has taken place, the solution in tank I0 ispermitted to cool and perhaps is diluted somewhat with water throughpipe 30 to raise the level of liquid to the desired point as shown bythe sight glasses 39. We are now ready for extraction.

Valves25 and 36 arenow closed and valves I1, 2|

and35are opened. The boiler I I is partially filled with a suitablesolvent such as ethyl ether or petroleum distillate, and heat is appliedto this boiler to causethe solvent therein to distill. The vapor passesthrough the vaporline I3 to condenser I2, where it condenses and passesdown through the pipe 22 emerging through the perforated coil 23 insmall droplets which pass upwards through the soap solution in tank Ithereby extracting the non-saponifiable constituents. This extract.

accumulates above the soap solution in the tank until it reaches thelevel of pipe I0 through which it flows over into the boiler H. Thesolvent continues to be volatilized and condensed performing its solventfunction until all extractible material has been removed andconcentrated in a relatively small amount of the solvent from which itmay be recovered by any well-known process.

During this entire time, the space in the upper portions of theapparatus not filled with materials being treated or by the solvent arefilled with nitrogen or other inert gas. In this way the material to berecovered, including particularly vitamins, is never in contact withoxygen and consequently may be recovered without loss of potency.

In Fig. 2 is shown a modification of the apparatus for the extraction ofnon-saponifiable matter by means of a solvent heavier than water. Thegeneral arrangement of treating tank H0, condenser II2, boiler I II andgas holder is much the same as in Fig. 1, but the connections and modeof operation are somewhat diflerent.

A boiler III is connected with a condenser II! by a relatively largevapor tube and the condenser is connected to a tank 0 by a reflux line II9. The treating tank is provided with a conical is connected to gasholder I3 with a pipe I24 and control valve I25. Communication betweenthe treating tank H0 and the gas holder is established with pipe I46leading into pipe I24 and fitted with valve I45. Provision for admittingliquids to tank H0 is made with pipe I30 and valve I3I, and for drainagethrough valve I32. Vapor line H8 is likewise provided with a vent H8 forthe same purpose as in Figure l.

The method of operation is as follows: The entire system is filled withnitrogen or other inert gas by first completely filling with water. Thiswater is drained off through valves I32 and I33; the emptying waterbeing replaced with gas from gas holder I I3 through pipe I24. When thisoperation is completed, oil to be treated, for example wheat germ oilcontaining vitamin E, is pumped into tank IIO through pipe I30 andfollowed by alkali solution in proper volume and proportion forsaponification. Steam is then introduced through coil I48 to heat themixture of oil and alkali solution until saponiflcation is completed.

During this operation valves I3I, I32, I33, I43,

II and I45 are closed, While valve I25 remains open. Any vapors evolvedfrom the boiling liquid in 0 pass upwards through H9 into condensertubes I20 where they are condensed to liquid and return to the reactionmixture through I I9. Pressure within the system is equalized andmaintained slightly in excess of atmospheric .by

- connection to the gas holder.

After saponiflcation is complete the solution in tank I I0 is allowed tocool and diluted with water admitted through pipe I30 until the volumeis satisfactory as indicated by sight glasses I33. Valve I25 is nowclosed and valves I40 and III opened. A suitable solvent 01' greaterdensity ,than water, such as for example carbon tetra- ,chlorlde ortrichlorethylene, is admitted to the boiler III through valve I33and-heat is applied through steam coil I30. The vaporized solventdistills through pipe I I0, condenses in condensing tubes I20 and flowsthrough pipe II! to the periorated distributing plate I41. From thisplate it falls in droplets through the soap solution dissolving andextracting part of the non-saponifiable matter in its passage andfinally accumulating in the lower portion I53 of tank IIO. When theinterface III between the two liquids has reached a suitable point asobserved through sight glasses I38, valve I49 is opened and the extractpermitted to fiow back to boiler III through pipes I50 and I52. Thefunction of valve III is to maintain pressure equilibrium between theboiler and extraction chamber in the event that condenser tubes I20become overloaded with solvent and completely fill up. Any suchvariation of pressure between the two parts of the system would resultin mechanical displacement of the levels I40 and HI and might cause thesoap solution to be forced over into the boiler.

The extraction process is continued until all the non-saponiflablematerial has been removed and concentrated in the relatively smallamount of solvent contained in the boiler. Recovery of thenon-saponiflable from this solution may be effected by known methods.

During the entire time required for introduction of materials,saponification, dilution, cooling and extraction, the vacant spaces ofthe apparatus are kept filled with nitrogen or other inert gas under asmall but constant pressure. In this way the material to be recovered isnever exposed to the action of oxygen, particularly while in contactwith alkaline soap solutions, a combination which results in rapiddestruction of vitamins, particularly vitamin E, with consequentreduction in potency of the concentrate desired.

While I have shown and described but two embodiments of my invention, itis to be understood that it is capable of many modifications. Changes,therefore, may be made which do not depart from the spirit and scope ofmy invention as disclosed in the appended claims.

I claim as my invention:

1. Apparatus for the saponification of a liquid and for the solventextraction of the non-saponifiable component thereof which comprises atank, heat exchange means for said tank, a still disposed separatelyfrom said tank, a. condenser, avapor conduit connecting the upper vaporportion of said condenser with the upper vapor portion of said still, aconduit for condensate connecting the lower portion of said condenserwith the upper portion of said tank, and a valved conduit connectionbetween the tank and the still, below said vapor conduit connection soarranged as to permit gravity return flow from said tank to said still.

2. Apparatus for the saponification of a liquid and for the solventextraction of the non-saponifiable component thereof which comprises atank, heat exchange means for said tank, a still disposed separatelyfrom'said tank, a condenser, a vapor conduit connecting the upper vaporportion of said condenser with the upper vapor portion of said still, aconduit for condensate connecting the lower portion of said condenserwith the upper portion of said tank, and a valved conduit connectionfrom the bottom of said tank to said still so arranged to permit gravityreturn flow from said tank to said still.

3. Apparatus for the saponiflcation of a liquid and for the solventextraction of the non-saponifiable component thereof which comprises atank, heat exchange means for said tank, a still disposed separatelyfrom said tank, a condenser, a vapor conduit connecting the upper vaporportion of said condenser with the upper vapor portion of said still, aconduit for condensate connecting the lower portion of said condenserwith the upper portion of said tank, conduit means extending from thebottom of said condenser-to the bottom of said tank, and valved conduitmeans near the top of said tank connecting said v and for thesolventextraction of the non-saponifiable component thereof which comprises atank, heat exchange means for said tank, a still disposed separatelyfrom said tank, a condenser, a vapor conduit connecting the upper vaporportion of said condenser with the upper vapor portion of said still, asource of inert gas, a conduit connecting said source and saidcondenser, a conduit for condensate connecting the lower portion of saidcondenser with the upper portion of said tank, and a valved conduitconnection between the tank and the still, .below said vapor conduitconnection so arranged as to permit gravity return flow from said tankto said still.

DONALD S. BINNINGTON.

